#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/40/7004032.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7004032
loop_
_publ_author_name
'Martínez-Lillo, José'
'Armentano, Donatella'
'Marino, Nadia'
'Arizaga, Livia'
'Chiozzone, Raúl'
'González, Ricardo'
'Kremer, Carlos'
'Cano, Joan'
'Faus, Juan'
_publ_section_title
;
 Pentachloro(pyrazine)rhenate(iv) complex as precursor of
 heterobimetallic pyrazine-containing ReIV2MII (M = Ni, Cu) species:
 synthesis, crystal structures and magnetic properties
;
_journal_issue                   34
_journal_name_full               'Dalton Transactions'
_journal_page_first              4585
_journal_paper_doi               10.1039/b802112k
_journal_year                    2008
_chemical_formula_sum            'C9 H16 Cl5 N4 Ni0.5 Re'
_chemical_formula_weight         573.06
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.765(3)
_cell_angle_beta                 83.256(3)
_cell_angle_gamma                72.767(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4084(7)
_cell_length_b                   8.5093(7)
_cell_length_c                   12.2145(12)
_cell_measurement_reflns_used    7469
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.263
_cell_measurement_theta_min      2.514
_cell_volume                     826.42(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'X8APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21013
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    8.704
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    2.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.374
_refine_diff_density_min         -1.442
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0215P)²+1.7662P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0542
_reflns_number_gt                3382
_reflns_number_total             3557
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b802112k.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C9 H16 Cl5 N4 Ni0.50 Re'
_cod_database_code               7004032
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 1.0000 0.0000 0.03944(16) Uani 1 2 d S . .
N3 N 0.3164(4) 0.9015(4) 0.0277(3) 0.0457(8) Uani 1 1 d . . .
H3B H 0.2482 0.9551 0.0839 0.055 Uiso 1 1 calc R . .
N4 N 0.6186(4) 0.8627(4) 0.1197(3) 0.0455(8) Uani 1 1 d . . .
H4B H 0.5698 0.9097 0.1834 0.055 Uiso 1 1 calc R . .
C5 C 0.3469(8) 0.7223(6) 0.0614(4) 0.0676(15) Uani 1 1 d . . .
H5A H 0.2403 0.6989 0.0790 0.081 Uiso 1 1 calc R . .
H5B H 0.4055 0.6594 -0.0002 0.081 Uiso 1 1 calc R . .
C6 C 0.4462(8) 0.6679(6) 0.1584(4) 0.0721(17) Uani 1 1 d . . .
H6A H 0.4540 0.5530 0.1802 0.087 Uiso 1 1 calc R . .
H6B H 0.3883 0.7319 0.2197 0.087 Uiso 1 1 calc R . .
C7 C 0.6194(7) 0.6864(6) 0.1363(4) 0.0652(15) Uani 1 1 d . . .
H7A H 0.6835 0.6333 0.1980 0.078 Uiso 1 1 calc R . .
H7B H 0.6740 0.6310 0.0708 0.078 Uiso 1 1 calc R . .
C8 C 0.7908(6) 0.8758(7) 0.1056(4) 0.0605(13) Uani 1 1 d . . .
H8A H 0.8575 0.8043 0.0501 0.073 Uiso 1 1 calc R . .
H8B H 0.8423 0.8436 0.1747 0.073 Uiso 1 1 calc R . .
C9 C 0.7794(6) 1.0504(7) 0.0699(4) 0.0607(13) Uani 1 1 d . . .
H9A H 0.7238 1.1200 0.1291 0.073 Uiso 1 1 calc R . .
H9B H 0.8905 1.0633 0.0517 0.073 Uiso 1 1 calc R . .
Re1 Re 0.908849(19) 0.706014(18) -0.289190(12) 0.03729(6) Uani 1 1 d . . .
Cl1 Cl 1.03259(17) 0.63969(16) -0.12449(10) 0.0647(3) Uani 1 1 d . . .
Cl2 Cl 0.64193(14) 0.75014(13) -0.19216(9) 0.0509(2) Uani 1 1 d . . .
Cl3 Cl 0.92754(17) 0.43192(13) -0.30742(10) 0.0570(3) Uani 1 1 d . . .
Cl5 Cl 1.16354(15) 0.67645(17) -0.39618(11) 0.0650(3) Uani 1 1 d . . .
Cl4 Cl 0.88549(15) 0.98812(13) -0.28053(9) 0.0512(2) Uani 1 1 d . . .
N1 N 0.7799(4) 0.7718(4) -0.4391(3) 0.0406(7) Uani 1 1 d . . .
N2 N 0.6016(6) 0.8703(5) -0.6259(3) 0.0584(10) Uani 1 1 d . . .
C1 C 0.6621(6) 0.7025(6) -0.4578(4) 0.0548(11) Uani 1 1 d . . .
H1 H 0.6387 0.6198 -0.4079 0.066 Uiso 1 1 calc R . .
C2 C 0.5760(7) 0.7537(7) -0.5504(4) 0.0634(13) Uani 1 1 d . . .
H2 H 0.4950 0.7036 -0.5608 0.076 Uiso 1 1 calc R . .
C3 C 0.8086(6) 0.8879(6) -0.5143(4) 0.0519(11) Uani 1 1 d . . .
H3 H 0.8905 0.9373 -0.5050 0.062 Uiso 1 1 calc R . .
C4 C 0.7189(7) 0.9364(6) -0.6060(4) 0.0588(12) Uani 1 1 d . . .
H4 H 0.7417 1.0191 -0.6560 0.071 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ni1 N4 180.000(1) . 2_675 ?
N4 Ni1 N3 92.75(16) . . ?
N4 Ni1 N3 87.25(16) 2_675 . ?
N4 Ni1 N3 87.25(16) . 2_675 ?
N4 Ni1 N3 92.75(16) 2_675 2_675 ?
N3 Ni1 N3 180.0 . 2_675 ?
C9 N3 C5 111.0(4) 2_675 . ?
C9 N3 Ni1 106.6(3) 2_675 . ?
C5 N3 Ni1 121.1(3) . . ?
C9 N3 H3B 105.7 2_675 . ?
C5 N3 H3B 105.7 . . ?
Ni1 N3 H3B 105.7 . . ?
C8 N4 C7 110.6(4) . . ?
C8 N4 Ni1 107.5(3) . . ?
C7 N4 Ni1 118.2(3) . . ?
C8 N4 H4B 106.7 . . ?
C7 N4 H4B 106.7 . . ?
Ni1 N4 H4B 106.7 . . ?
C6 C5 N3 112.8(4) . . ?
C6 C5 H5A 109.0 . . ?
N3 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
N3 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
C5 C6 C7 113.1(4) . . ?
C5 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
N4 C7 C6 112.3(4) . . ?
N4 C7 H7A 109.2 . . ?
C6 C7 H7A 109.2 . . ?
N4 C7 H7B 109.2 . . ?
C6 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
N4 C8 C9 106.8(4) . . ?
N4 C8 H8A 110.4 . . ?
C9 C8 H8A 110.4 . . ?
N4 C8 H8B 110.4 . . ?
C9 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
N3 C9 C8 108.2(4) 2_675 . ?
N3 C9 H9A 110.1 2_675 . ?
C8 C9 H9A 110.1 . . ?
N3 C9 H9B 110.1 2_675 . ?
C8 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
N1 Re1 Cl1 177.03(9) . . ?
N1 Re1 Cl3 88.28(10) . . ?
Cl1 Re1 Cl3 92.13(5) . . ?
N1 Re1 Cl5 89.51(10) . . ?
Cl1 Re1 Cl5 93.43(6) . . ?
Cl3 Re1 Cl5 90.21(6) . . ?
N1 Re1 Cl2 86.54(10) . . ?
Cl1 Re1 Cl2 90.50(5) . . ?
Cl3 Re1 Cl2 91.60(5) . . ?
Cl5 Re1 Cl2 175.61(4) . . ?
N1 Re1 Cl4 88.69(10) . . ?
Cl1 Re1 Cl4 90.93(5) . . ?
Cl3 Re1 Cl4 176.90(4) . . ?
Cl5 Re1 Cl4 89.08(5) . . ?
Cl2 Re1 Cl4 88.89(5) . . ?
C3 N1 C1 116.9(4) . . ?
C3 N1 Re1 121.5(3) . . ?
C1 N1 Re1 121.6(3) . . ?
C2 N2 C4 114.9(4) . . ?
N1 C1 C2 120.1(4) . . ?
N1 C1 H1 119.9 . . ?
C2 C1 H1 119.9 . . ?
N2 C2 C1 123.9(5) . . ?
N2 C2 H2 118.1 . . ?
C1 C2 H2 118.1 . . ?
N1 C3 C4 121.2(4) . . ?
N1 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
N2 C4 C3 123.0(4) . . ?
N2 C4 H4 118.5 . . ?
C3 C4 H4 118.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N4 1.944(3) . ?
Ni1 N4 1.944(3) 2_675 ?
Ni1 N3 1.945(3) . ?
Ni1 N3 1.945(3) 2_675 ?
N3 C9 1.471(6) 2_675 ?
N3 C5 1.489(6) . ?
N3 H3B 0.9100 . ?
N4 C8 1.473(6) . ?
N4 C7 1.490(6) . ?
N4 H4B 0.9100 . ?
C5 C6 1.483(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.500(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.480(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N3 1.471(6) 2_675 ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
Re1 N1 2.174(3) . ?
Re1 Cl1 2.3120(13) . ?
Re1 Cl3 2.3241(12) . ?
Re1 Cl5 2.3350(14) . ?
Re1 Cl2 2.3570(13) . ?
Re1 Cl4 2.3629(11) . ?
N1 C3 1.331(5) . ?
N1 C1 1.346(6) . ?
N2 C2 1.327(7) . ?
N2 C4 1.328(7) . ?
C1 C2 1.376(7) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 C4 1.380(6) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
